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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 55 records · Page 3

Failure of morphology of (0 deg)8 graphite/epoxy as influenced by environments and processing

Optical and scanning electron microscopy were used to investigate the failure morphology of graphite/epoxy specimens which had been tested until tensile failure. Failure morphology was studied as a function of the quality control variables of specimen preparation technique, prepreg batch, and cure condition, and also as a function of the environmental parameters of temperature and moisture content. Defective specimens were found to exhibit a low energy failure morphology. Poor specimen edge preparation and one batch of prepreg when tested at elevated temperature or moisture content also exhibited energy failure morphology. Postcuring had no effect on strength but did slightly alter failure morphology. Temperature or moisture appeared to decrease flaw sensitivity and thus increase strength; however, moisture also appeared to increase interfacial debonding between filament and matrix. When combined moisture and temperature increased interfacial debonding and made the epoxy matrix more prone to fracture.

Clements, L. L.↗

Characterization of Molybdate Conversion Coatings for Aluminum Alloys by Electrochemical Impedance Spectroscopy

Electrochemical impedance spectroscopy (EIS) was used to investigate the corrosion inhibiting properties of newly developed proprietary molybdate conversion coatings on aluminum alloy 2024-T3 under immersion in aerated 5% (w/w) NaCl. Corrosion potential and EIS measurements were gathered for six formulations of the coating at several immersion times for two weeks. Nyquist as well as Bode plots of the data were obtained. The conversion-coated alloy panels showed an increase in the corrosion potential during the first 24 hours of immersion that later subsided and approached a steady value. Corrosion potential measurements indicated that formulations A, D, and F exhibit a protective effect on aluminum 2024-T3. The EIS spectra of the conversion-coated alloy were characterized by an impedance that is higher than the impedance of the bare alloy at all the immersion times. The low frequency impedance, Z(sub lf) (determined from the value at 0.05 Hz) for the conversion-coated alloy was higher at all the immersion times than that of the bare panel. This indicates improvement of corrosion resistance with addition of the molybdate conversion coating. Scanning electron microscopy (SEM) revealed the presence of cracks in the coating and the presence of cubic crystals believed to be calcium carbonate. Energy dispersive spectroscopy (EDS) of the test panels revealed the presence of high levels of aluminum, oxygen, and calcium but did not detect the presence of molybdenum on the test panels. X-ray photoelectron spectroscopy (XPS) indicated the presence of less than 0.01 atomic percent molybdenum on the surface of the coating.

Calle, Luz Marina↗

Sequentially evaporated thin Y-Ba-Co-O superconducting films on microwave substrates

The development of high T sub c superconducting thin films on various microwave substrates is of major interest in space electronic systems. Thin films of YBa2Cu3O(7-Delta) were formed on SrTiO3, MgO, ZrO2 coated Al2O3, and LaAlO3 substrates by multi-layer sequential evaporation and subsequent annealing in oxygen. The technique allows controlled deposition of Cu, BaF2 and Y layers, as well as the ZrO buffer layers, to achieve reproducibility for microwave circuit fabrication. The three layer structure of Cu/BaF2/Y is repeated a minimum of four times. The films were annealed in an ambient of oxygen bubbled through water at temperatures between 850 C and 900 C followed by slow cooling (-2 C/minute) to 450 C, a low temperature anneal, and slow cooling to room temperature. Annealing times ranged from 15 minutes to 5 hrs. at high temperature and 0 to 6 hr. at 450 C. Silver contacts for four probe electrical measurements were formed by evaporation followed with an anneal at 500 C. The films were characterized by resistance-temperature measurements, energy dispersive X-ray spectroscopy, X-ray diffraction, and scanning electron microscopy. Critical transition temperatures ranged from 30 K to 87 K as a function of the substrate, composition of the film, thicknesses of the layers, and annealing conditions. Microwave ring resonator circuits were also patterned on these MgO and LaAlO3 substrates.

Valco, G. J.↗

Corrosion Behavior of Stainless Steel 304 and Nickel 625 Under Iodine Vapor at 300 °C

The chemical, structural, and microstructural behavior of stainless steel 304 (SS 304) and nickel 625 (Ni 625) were probed after exposure to iodine vapor laminar flow at 300 °C. This work was conducted in support of the development of in-space propulsion utilizing iodine as a propellant. The kinetics of corrosion was measured in a custom-built iodine-compatible thermogravimetric analyzer rig at 300 °C in which samples were exposed to an iodine laminar vapor flow of 1 mg/min (carried by 20 mL/min argon gas) for up to 31 days. Samples were characterized after the experiment by X-ray diffraction, electron microscopy, energy dispersive X-ray spectroscopy, and dynamic secondary ion mass spectrometry. All samples formed scales consisting mainly of metal oxyiodides showing different chemistry, microstructure, and crystalline phases. The paralinear rate law best describes the kinetics of oxidation of the samples. SS 304 exhibited slightly slower kinetics of oxidation (106±3·10(exp –5) mg/sq.cm/day) than Ni 625 (122±3·10(exp –5) mg/sq.cm/day) in the low-oxygen and low-water environment.

Chemistry and Materials↗

Investigation into Interfacial Mixing Behavior of Blown Powder Deposited Inconel 625-Copper Alloy Bimetallic for Improvement of Bimetallic Joint Strength

Use of laser blown powder, directed energy deposition (DED) provides a method for fabrication of bimetallic functional materials for high heat flux applications. However, this relatively new process currently has a low technology readiness level (TRL). Key to increasing the TRL is a better understanding of the factors that control mixing of the bi-metallic materials at the interface. The resulting interfaces in specimens obtained from three vendors were characterized using optical and electron microscopy with electron dispersion spectroscopy in addition to mechanical testing. Based on the range of process parameters and resulting interfaces, a model is being developed to predict interfacial mixing for development of specifications for improved and repeatable microstructures.

Additive Manufacturing↗

Corrosion of 310 stainless steel in H2-H2O-H2S gas mixtures: Studies at constant temperature and fixed oxygen potential

Corrosion of SAE 310 stainless steel in H2-H2O-H2S gas mixtures was studied at a constant temperature of 1150 K. Reactive gas mixtures were chosen to yield a constant oxygen potential of approximately 6 x 10 to the minus 13th power/cu Nm and sulfur potentials ranging from 0.19 x 10 to the minus 2nd power/cu Nm to 33 x 10 to the minus 2nd power/cu Nm. The kinetics of corrosion were determined using a thermobalance, and the scales were analyzed using metallography, scanning electron microscopy, and energy dispersive X-ray analysis. Two corrosion regimes, which were dependent on sulfur potential, were identified. At high sulfur potentials (p sub S sub 2 less than or equal to 2.7 x 10 to the minus 2nd power/cu Nm) the corrosion rates were high, the kinetics obeyed a linear rate equation, and the scales consisted mainly of sulfide phases similar to those observed from pure sulfication. At low sulfur potentials (P sub S sub 2 less than or equal to 0.19 x 10 to the minus 2nd power/cu Nm) the corrosion rates were low, the kinetics obeyed a parabolic rate equation, and scales consisted mainly of oxide phases.

Rao, D. B.↗

Characterization of Cosmic Grain Analogs Formed at Low Temperature from Small Hydrocarbon Precursors in the NASA Ames COSmIC Facility

Here, we present the results of the first solid-phase ex situ analysis of cosmic grain analogs produced at low temperature (<200 K) in the NASA Ames COsmic SImulation Chamber (COSmIC) from small hydrocarbon precursors, methane (CH4) and acetylene (C2H2), seeded in an argon supersonic jet expansion and submitted to a plasma discharge. The plasma-induced chemical reactions, initiated between the precursor molecules and their atomic and molecular fragments, radicals and ions, produce larger molecules and eventually solid particles that are collected in situ under controlled conditions. Scanning electron microscopy (SEM) imaging was used to provide insight on the morphology and growth structure of the grains produced in COSmIC, and to investigate how the precursors used to produce the grains affect these parameters. This SEM study has shown that under identical experimental conditions with fixed physical and chemical parameters (precursor density, temperature, energy, and reaction time), heavier precursors in the initial mixture produce larger grains and in larger quantity, most likely as a result of a more complex chemistry: most of the grains produced in the Ar/CH4 (95:5) gas mixture ranged from 15 to 385 nm in diameter with an average density of 2.1 grains per sq.μm, while the grains produced in the Ar/C2H2 (95:5) gas mixture ranged from 40 to 650 nm with a density of 3.5 grains per sq.μm. Changes in the morphology were also observed, with grains produced from acetylene (C2H2) precursors tending to be more spherical than grains produced from methane (CH4) precursors. This change in morphology could be associated with different stages of growth formation at low temperature from a more "planar" growth at first, followed by coagulation into more spherical particles. This study demonstrates that the COSmIC experimental setup can be used to investigate carbon grain formation from small gas-phase molecular precursors at low temperature (<200 K), i.e., under a temperature regime that is representative of the dust condensation zone and outer region of circumstellar envelopes.

Ella Sciamma-O'Brien↗

Electron energy loss spectroscopy techniques for the study of microbial chromium(VI) reduction

Electron energy loss spectroscopy (EELS) techniques were used to determine oxidation state, at high spatial resolution, of chromium associated with the metal-reducing bacteria, Shewanella oneidensis, in anaerobic cultures containing Cr(VI)O4(2-). These techniques were applied to fixed cells examined in thin section by conventional transmission electron microscopy (TEM) as well as unfixed, hydrated bacteria examined by environmental cell (EC)-TEM. Two distinct populations of bacteria were observed by TEM: bacteria exhibiting low image contrast and bacteria exhibiting high contrast in their cell membrane (or boundary) structure which was often encrusted with high-contrast precipitates. Measurements by EELS demonstrated that cell boundaries became saturated with low concentrations of Cr and the precipitates encrusting bacterial cells contained a reduced form of Cr in oxidation state + 3 or lower.

Evaluation Studies↗

Focused Ion Beam Recovery of Hypervelocity Impact Residue in Experimental Craters on Metallic Foils

The Stardust sample return capsule will return to Earth in January 2006 with primitive debris collected from Comet 81P/Wild-2 during the fly-by encounter in 2004. In addition to the cometary particles embedded in low-density silica aerogel, there will be microcraters preserved in the Al foils (1100 series; 100 micrometers thick) that are wrapped around the sample tray assembly. Soda lime spheres (approximately 49 m in diameter) have been accelerated with a light-gas-gun into flight-grade Al foils at 6.35 km s(sup -1) to simulate the potential capture of cometary debris. The preserved crater penetrations have been analyzed using scanning electron microscopy (SEM) and x-ray energy dispersive spectroscopy (EDX) to locate and characterize remnants of the projectile material remaining within the craters. In addition, ion beam induced secondary electron imaging has proven particularly useful in identifying areas within the craters that contain residue material. Finally, high-precision focused ion beam (FIB) milling has been used to isolate and then extract an individual melt residue droplet from the interior wall of an impact penetration. This enabled further detailed elemental characterization, free from the background contamination of the Al foil substrate. The ability to recover pure melt residues using FIB will significantly extend the interpretations of the residue chemistry preserved in the Al foils returned by Stardust.

Graham, G. A.↗

Surface Chemistry, Friction, and Wear Properties of Untreated and Laser-Annealed Surfaces of Pulsed-Laser-Deposited WS(sub 2) Coatings

An investigation was conducted to examine the surface chemistry, friction, and wear behavior of untreated and annealed tungsten disulfide (WS2) coatings in sliding contact with a 6-mm-diameter 440C stainless-steel ball. The WS2 coatings and annealing were performed using the pulsed-laser-deposition technique. All sliding friction experiments were conducted with a load of 0.98 N (100 g), an average Hertzian contact pressure of 0.44 GPa, and a constant rotating speed of 120 rpm. The sliding velocity ranged from 31 to 107 mm/s because of the range of wear track radii involved in the experiments. The experiment was performed at room temperature in three environments: ultrahigh vacuum (vacuum pressure, 7X(exp -10) Pa), dry nitrogen (relative humidity, less than 1 percent), and humid air (relative humidity, 15 to 40 percent). Analytical techniques, including scanning electron microscopy (SEM), energy-dispersive x-ray spectroscopy (EDX), x-ray photo electron spectroscopy (XPS), surface profilometry, and Vickers hardness testing, were used to characterize the tribological surfaces of WS2 coatings. The results of the investigation indicate that the laser annealing decreased the wear of a WS2 coating in an ultrahigh vacuum. The wear rate was reduced by a factor of 30. Thus, the laser annealing increased the wear life and resistance of the WS2 coating. The annealed WS 2 coating had a low coefficient of friction (less than O.1) and a low wear rate ((10(exp -7) mm(exp 3)/N-m)) both of which are favorable in an ultrahigh vacuum.

Miyoshi, Kazuhisa↗

Lubrication with sputtered MoS2 films.

Sputtered MoS2 films (2000-6500 A) were deposited on highly polished metal surfaces. These films have a low coefficient of friction (0.03-0.04) at speeds of 40-80 rpm and loads of 250-1000 grams. At loads of 250 grams the wear lives are over 0.5 million cycles, but at 1000 gram loads, it decreases to 38,000 cycles. Friction experiments and tensile tests have indicated that sputtered films have a strong adherence to metal surfaces. Electron transmission, diffraction and scanning electron microscopy show that these films have an extremely small particle size, less than 30 A in diameter, and are very dense and free from observable pinholes. The high kinetic energy of these sputtered species, the submicroscopic particle size and the sputter-etched substrate surface is responsible for strong adhesion and cohesion of the sputtered film.

Spalvins, T.↗

Enhanced TiO2 Photocatalytic Processing of Organic Wastes for Green Space Exploration

The effect of transition metal co-catalysts on the photocatalytic properties of TiO2 was investigated. Ruthenium (Ru), palladium, platinum, copper, silver, and gold, were loaded onto TiO2 powders (anatase and mixed-phase P25) and screened for the decomposition of rhodamine B (RhB) under broad-band irradiation. The morphology and estimated chemical composition of photocatalysts were determined by scanning electron microscopy and energy dispersive spectroscopy, respectively. Brunhauer, Emmett and Teller (BET) analysis measured mass-specific surface area(s). X-ray diffraction analysis was performed to confirm the identity of titania phase(s) present. The BET surface area of anatase TiO2/Ru 1% (9.2 sq m/gm) was one of the highest measured of all photocatalysts prepared in our laboratory. Photolyses conducted under air-saturated and nitrogen-saturated conditions revealed photodegradation efficiencies of 85 and 2 percent, respectively, after 60 min compared to 58 percent with no catalyst. The cause of low photocatalytic activity under an inert atmosphere is discussed. TiO2/Ru 1% showed a superior photocatalytic activity relative to P25-TiO2 under broad-band irradiation. A potential deployment of photocatalytic technologies on a mission could be a reactor with modest enhancement in solar intensity brought about by a trough-style reactor, with reactants and catalyst flowing along the axis of the trough and therefore being illuminated for a controlled duration based on the flow rate.

Udom, I.↗

Non-Protein Amino Acids Identified in Carbon-Rich Hayabusa Particles

Amino acid abundances in acid-hydrolyzed hot water extracts of gold foils containing five Category 3 (carbon-rich) Hayabusa particles were studied using liquid chromatography with tandem fluorescence and accurate mass detection. Initial particle analyses using field emission scanning electron microscopy with energy-dispersive X-ray spectrometry indicated that the particles were composed mainly of carbon. Prior to amino acid analysis, infrared and Raman microspectroscopy showed some grains possessed primitive organic carbon. Although trace terrestrial contamination, namely L-protein amino acids, was observed in all Hayabusa extracts, several terrestrially uncommon non-protein amino acids were also identified. Some Hayabusa particles contained racemic (D≈L) mixtures of the non-protein amino acids β-aminoisobutyric acid (β-AIB) and β-amino-n-butyric acid (β-ABA) at low abundances ranging from 0.09 to 0.31 nmol g −1 . Larger abundances of the non-protein amino acid β-alanine (9.2 nmol g −1 , ≈4.5 times greater than background levels) were measured in an extract of three Hayabusa particles. This β-alanine abundance was ≈6 times higher than that measured in an extract of a CM2 Murchison grain processed in parallel. The comparatively high β-alanine abundance is surprising as asteroid Itokawa is similar to amino acid-poor LL ordinary chondrites. Elevated β-alanine abundances and racemic β-AIB and β-ABA in Hayabusa grains suggested these compounds have non-biological and plausibly non-terrestrial origins. These results are the first evidence of plausibly extraterrestrial amino acids in asteroid material from a sample-return mission and demonstrate the capabilities of the analytical protocols used to study asteroid Ryugu and Bennu samples returned by the JAXA Hayabusa2 and NASA OSIRIS-REx missions, respectively.

Eric T. Parker↗

An unusual layered mineral in chondrules and aggregates of the Allende carbonaceous chondrite

Transmission electron microscopy (TEM), scanning electron microscopy (SEM), and energy dispersive X ray (EDS) and electron energy loss (EELS) spectroscopy examinations of the microstructures and phase relationships of minerals in opaque spherules in the Allende chondrules and aggregates are reported. The studies were carried out on petrographic thin sections which were ion-thinned. A significant metasomatic effect was observed in a highly oxidizing condition of a later cooled stage. An unusually layered Fe-, Ni-, and O-rich mineral related to serpentine was found to occur in the opaque specimen, and was judged to occur by alteration of olivine. It is noted that low temperature and a hydrous condition would have been required for the formation of the serpentine in the spherules, the first observed in Allende. It is suggested that the aqueous conditions occurred before the final stage of the meteorite formation, and proceeded in a nonterrestrial manner.

Tomeoka, K.↗

In situ transmission electron microscopy study on the epitaxial growth of CoSi2 on Si(111) at temperatures below 150 C

This paper reports an in situ transmission electron microscopy study on the epitaxial growth of CoSi2 on Si(111) from a 10-nm-thick amorphous mixture of Co and Si in the ratio 1:2, which was formed by codeposition of Co and Si near room temperature. Nuclei of CoSi2 are observed in the as-deposited film. These nuclei are epitaxial and extend through the whole film thickness. Upon annealing, these columnar epitaxial CoSi2 grains grow laterally at temperatures as low as 50 C. The kinetics of this lateral epitaxial growth was studied at temperatures between 50 and 150 C. The activation energy of the growth process is 0.8 + or - 0.1 eV.

Nieh, C. W.↗

Irradiation Effects in Fosterrite and the Nature of Interstellar Grains: A Coordinated Spectroscopy and Electron Microscopy Study

Crystalline and amorphous silicates condense in the outflows of low mass evolved stars and massive red supergiant stars and are injected into the interstellar medium (ISM) where they are rendered almost completely amorphous by a multitude of destructive processes (e.g. shock, grain-grain collisions, and irradiation). Irradiation effects in particular may have played an important role in the genesis and modification of primitive grains in cometary dust, but unraveling those effects requires controlled experiments under appropriate conditions and with an emphasis on materials relevant to the ISM. Here we report our infrared (IR) microspectroscopy and trans-mission electron microscope (TEM) measurements on forsterite that was amorphized through irradiation by high energy heavy ions.

Keller, Lindsay P.↗

Producing Zirconium Diboride Components with Complex, Near-Net Shape Geometries by Aqueous Room-Temperature Injection Molding

Room-temperature injection molding is proposed as a novel, low-cost and more energy efficient manufacturing process capable of forming complex-shaped zirconium diboride (ZrB2) parts. This innovative processing method utilized aqueous suspensions with high powder loading and a minimal amount (5 vol.) of water-soluble polyvinylpyrrolidone (PVP), which was used as a viscosity modifier. Rheological characterization was performed to evaluate the room-temperature flow properties of ZrB2-PVP suspensions. ZrB2 specimens were fabricated with high green body strength and were machinable prior to binder removal despite their low polymer content. After binder burnout and pressureless sintering, the bulk density and microstructure of specimens were characterized using Archimedes technique and scanning electron microscopy. X-Ray Diffraction was used to determine the phase compositions present in sintered specimens. Ultimate strength of sintered specimens will be determined using ASTM C1323-10 compressive C-ring test.

Near-Net Shape Forming↗

Advanced TUFROC Thermal Protection System Evolution Under Re-entry like Conditions

Toughened Unipiece Fibrous Reinforced Oxidation-resistant Composite (TUFROC) and its successor, Advanced TUFROC, are state-of-the-art thermal protection systems (TPS) for high temperature reusable applications. Originally designed for use on the wing-leading edge of X-37B, TUFROC is an insulative tiled system consisting of a low-conductivity ceramic base, a carbonaceous cap, and multiple coatings for thermal performance. The improved Advanced TUFROC has demonstrated reusability up to 2900 °F and single use capabilities exceeding 3200 °F. This effort explores the evolution of Advanced TUFROC when exposed to re-entry like conditions via arc jet testing. Chemical reactions and constituent migration resulting from the aerothermal heating are known to occur and are studied in detail. Further, the interaction between the multiple constituents and layers will be discussed as this is believed to have a significant impact on the overall performance. Characterization includes structural analysis via optical microscopy, scanning electron microscopy and energy-dispersive x-ray spectroscopy.

Thermal protection system↗